HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(3-Chlorophenyl)piperazine monohydrochloride → 8-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(3-Chlorophenyl)piperazine monohydrochloride | HCID 25681 | — |
| Reactant | 8-(3-Bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione | HCID 14280583 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 8-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate | HCID 131715732 | — |
Reaction Steps
A solution of 8-(3-bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione (4.0 g) and 1-(3-chlorophenyl)piperazine hydrochloride (3.06 g) in 50 ml of Et3N was heated to reflux with stirring under N2. After 1 hour TLC (thin layer chromatography) showed the absence of starting material. The excess Et3N was removed in vacuo and the residue chromatographed on silica using ethyl acetate as the eluent. Fractions containing the desired product were combined and concentrated in vacuo.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04826846 |
| Source dataset | uspto-grants-1989_05 |
| ORD ID | ord-c55a9c5047b041e78a0ff6d57ab68f58 |
| Source note | uspto-grants-1989_05 |